( Reaffirmed 2012 ) IS : 9406 = 1980 Indian Standard SPECIFICATION FOR CALCIUM SILICATE FOR RUBBER Rubber Chairman DR D. BANE~JEE Members Ministry of Dafence ( R & D ) DR L. D. KANDPAL ( Alternate ) Ministry of Defence ( DGI ) SHRI A. K. BANDOPADHAYA SHRI B. C. SEN ( Alternate) Directorate General of Supplies & Disposals, SHRI A. T. BASAE New Delhi Indian Petrochemicals Corporation Ltd, Vadodara DR S. K. BEATNAOAR SHRI S. K. MAHESHWARI ( Alfernale ) National Test House, Calcutta SRRI S. K. BOSE SHRI A. GHOSH ( Alternate ) Bayer ( India ) Ltd, Bombay DR S. N. CEARRAVARTY SHRI R. R. PANDIT ( Alternate ) Alkali & Chemical Corporation of India Ltd, SHRI D. K. CHATTERJEE Rishra DR S. K. ROY ( Alternate ) Export Inspection Council of India, Calcutta SERI 0. P. DHAMIJA SHRI P. K. CEATTERJEE ( Alternate) Dunlop India Ltd, Calcutta SHRI S. B. GANUULI SHRI P. N. S. MYER ( Alternate ) Madras Rubber Factoty Ltd, Madras San1 A. GEORGE JOHN SHRI K. J: ABRAHAM ( Alternate ) Cosmos India Rubber Works Pvt Ltd, Bombay SRRI LALIT MOHAN JAMNADAS SHRI PULIN L. KINARIWALA ( Alternate ) Indian Oil Corporation Ltd, Bombay SHRI R. C. JHINGAN SHRI M. K. JAIN ( Alfernate ) National Rubber Manufacturers' Ltd, Calcutta DR I. V. KRISHNAMURTI SHRI R. P. MATEUR ( Alternate ) Lathia Rubber Manufacturing Co Pvt Ltd, Bombay SHRI S. V. LATHIA SHRI D. P. LATHIA ( Alternate ) Railway Board ( Ministry of Railways ) DR S. P. MAIUK SBRI D. N. V. CEELLAM ( Alfernate) SHRI M. L. BEHRANI INDUSTRY 13 Products Sectional Committee, PCDC Representing Escon Consultants Pvt Ltd, Calcutta ( Continued on page 2 ) INDIAN @ Copyrighr 1980 STANDARDS INSTITUTION This publication is protected under the Indian Copyright Act ( XIV of 1957 ) and reproduction in whole or in part by any means except with written permirsion of the publisher shall be deemed to be an infringement of copyright under the said Act. IS : 9406 - 1980 ( Continurd from pagr 1 ) Mcmbrrs Representing Indian Rubber Manufacturers' Research Association, Bombav Rubber B&d, Kottayam DR C. K. N. NAIR Sundaram Industries Pvt Ltd, Madras SHRI N. NAQARAJIN SHRI P. VIJAYARA~HAVAN ( Alternote ) Bata India Ltd, Calcutta SHRI S. C. NANDY SHRI SUNIL SARXAR ( Alternate ) Synthetics and Chemicals Lrd, Bombay SHRI M. M. PATEL Directorate General of Technical Development, DR N. V. C. RAO New Delhi SHHI G. R. INAMUAR ( Alternate ) All India Rubber Industries Association, Bombay SERI B. B. SANQTANI SHRI V. N. MAKAR ( Alternate ) Director General, IS1 ( Ex-oficio Member ) SHRI M. S. SAXENA. Director ( P & C j DR W. MILLN~ Secretary SHRI SATISR CEANDER Deputy Director ( P & C ), IS1 Rubber Chemicals Convener and Compounding Ingredients PCDC 13:5 Escon Consultants Subcommittee, SHRI A. K. SEN CHAUDHURI Pvt Ltd, Calcutta Members Bayer ( India ) Ltd, Bombay DR M. C. BADRINARAYANA DR S, N. CHAERAVARTY ( Alfernate ) Ministry of Defence ( DGI ) SHRI A. K. BANDOPADEYA SHRI p. L. NAQ ( Alternate ) Indian Rubber Manufacturers' Research Association, SERI B. BANERJEE Bombay Inchek Tyres Ltd, Calcutta SHRI B. BHATTACHARYA SERI P. K. SARKAR ( Alternate) National Test House, Calcutta SHRI S. K. BOSE Dn D. K. DAS ( Alternate ) Alkali & Chemical Corporation of India Ltd, SHRI D. K. CHATTERJEE Rishra DR S. K. RAY ( Alternate) United Carbon India Ltd, Bombay SERI R. W. DHARWADKAR Dunlop India Ltd, Calcutta SHRI S. B. GANQULI SHRI A. SIN ( Alternate ) All India Rubber Industries Association, Bombay; DR A. S. GHAQ and Mindia Chemicals Ltd, Bombay All India Rubber Industries Association, Bombay SHRI S. V. LATHIA ( Alternate I ) Mindia Chemicals Ltd, Bombay SEIRI H. B. KINQ~LEY ( Alternate II ) ( Continued on page 10 ) 2 IS : 9406 l 1980 Indian Standard SPECIFICATION FOR CALCIUM SILICATE FOR RUBBER INDUSTRY 0. 0.1 This Indian FOREWORD Standard was adopted by the Indian Standards Institution on 5 January 1980, after the draft finalized by the Rubber Products Sectional Committee had been approved by the Petroleum, Coal and Related Products Division Council. It is, however, essential that it 0.2 Calciumsilicateisan important filler. should be of proper quality so that through it no unwarranted impurities are added to the vulcanizate. 0.3 This standard contains clauses 2.3 and 3.1 which between the purchaser and the supplier. call for agreement 0.4 For the purpose of deciding whether a particular requirement of this or calculated, standard is complied with, the final value, observed expressing the result of a test or analysis, shall be rounded off in accorThe number of significant places retained in dance with IS : 2-1960.. the rounded off value should be the same as that of the specified value in this standard. 1. SCOPE 1.1 This standard prescribes the requirements and test for calcium silicate for rubber industry. 2. REQUIREMENTS 2.1 Description - The material shall be white amorphous shall be dry and free from extraneous impurities and grit. Table and methods of sampling powder. It in 2.2 The material shall also comply with the requirements laid down 1, when tested according to the method indicated against each. *Rules for rounding off numerical values ( r&cd ). 3 I6,:9406- 1980 TABLE 1 REO.UIREMBNTS FOR CALCIUM RUBBER INDUSTRY ( Clausa 2.2 ) SILICATE FOR 2. (1) i) ii) Bulk density, Sieve residue, Max a) Through Sieve b) Through Sieve c) Through Sieve iii) iv) v) vi) vii) viii) ix) x) xi) xii) xiii) Relative PH Moisture mass Matter cent density content, soluble by mass, ignition, REQUIREMENT METHOD or TEST, REF TO A_-c-eCl No. in ' ' Appendix IS : 7086 ( Part I )1973* (4) (5) 3 (2) g/ml percent by mass, IS IS IS (3) 0.16 f 0.03 A 53-micron 75.micron 150.micron 27/2X7 percent in water, Max percent 5 2 1 1.97 f 0.05 4 5 7 1.5 8 10 11 12 B C D 14 - 8 to 9 by perby 3.5 * 0'5 0.5 12 * Loss on mass Manganese by mass, Co::;; ( as Mn ), percent Max ), percent by by by by 0'001 2 0'0018 0~001 18 &2 68 f 130 f 4 10 (asxcu , Lead ( aa Pb ), percent mass, Max Ca~~tsmM~Xidc, Silica [as mass SiO, percent ), percent Oil absorption, g of linseed oil per 100 g of the material Sedimentation toluenc, ml Retention percent b) After *Methods volume in xiv) xv) 15* 1 E F - in suspension, by mass, Mix 80 60 and test for rubber compounding 20 minutes al After 5 minutes of sampling ingredients, Part I. 4 IS : 9406 - 1999 2.3 Compounding Test - may be compounded properties of calcium 3. PACKING AND If desired by the purchaser, the material in styrene butadiene rubber test recipe and the silicate compared with the approved sample. ' MARKING 3.1 Packing -The material shall be packed in polyethylene lined hessian bags laminated with bitumen or in suitable containers as agreed to between the purchaser and the supplier. 3.2 Marking - The bags or the containers, marked with the following: as the case may be, shall be 4 b) 4 4 Name of the material; name or trade-mark, and if any; Manufacturer's Net mass of the material; Month and year of manufacture. bags or the Mark. containers may also be marked with the IS1 3.2.1 The Certification NOTE - The use the ISI Certification Mark is governed by the provisions of the Indian Standards Institution ( Certification Marks ) Act and the Rules and Rcgulations made thereunder. The IS1 Mark on products covered by an Indian Standard conveys the assurance that they have been produced to comply with the requirements ofthat standard under a well-defined system of inspection, testing and quality control which is devised and supervised by IS1 and operated by the producer. IS1 marked products are also continuously checked by IS1 for conformity to that standard as a further safeguard. Details of conditions under which a licence for the use of the IS1 Certification Mark may be granted to manufacturers or processors, may be obtained from the Indian Standards Institution. 4. SAMPLING AND CRITERIA FOR shall CONFORMITY be done' as prescribed in 15 of 4.1 Sampling - The sampling IS : 7086 ( Part I )-1973*. 4.2 Number of Tests and Criteria for Conforming - Tests for all characteristics shall be conducted on composite sample. The lot shall be considered as conforming to the specification if the composite sample satisfies each of these requirements. *Methods of sampling and test for rubber compounding ingredient, Part I. 5 1s I 9406 - 1980 APPENDIX [ Table 1, Item DETERMINATION A-l. APPARATUS A (i) ] OF BULK DENSITY A-l.1 Assemble the apparatus as shown in Fig. 1. The base of the measuring cylinders A shall be ground flat and the empty measuring cylinder A together with the rubber bung shall weigh 250 f 5 g. It shall be accurately calibrated to 250 ml with an error, if any, of less than 1 ml. The distance between zero and 250-ml graduation on the measuring cylinder A shall be not less than 220 mm and not more than 240 mm. The distance between the flatground part of the base of the measuring cylinder A and the rubber base pad B, when the measuring cylinder A is raised to the full height shall be 25 f 2 mm. 180 - All dimensions in millimetres. h. 1 APPARATUS FOR THE DETERMINATION Base Pad The rubber OF BULK DENSITY A-1.2 Rubber base pad B shall have a hardness of 42 to 50 IRHD. A-l.3 Balance - Pans of the balance shall be at least 10 cm in diameter and the balance shall be sensitive to less than 0'1 g. 6 IS : 9406 - 1980 A-2. PROCEDURE A-2.1 Sieve about 40 g of the material through 250-micron IS Sieve on to a tared glazed paper and weigh it accurately. Slip the powder gently and smoothly into the measuring cylinder which should be held at 45" to the vertical, without knocking or squeezing. Assemble the apparatus as shown in Fig. 1. With the thumb and four fingers of one hand, gently grasp the upper part of the cylinder, and within one second lift it about 25 mm ( taking a care not to jerk the cylinder by knocking it against the upper stop ) and let it drop. Continue lifting and dropping until 50 complete drops have been given to the cylinder. During this operation give a gentle turn of about 10" in the clockwise direction to the cylinder after every two drops. As soon as 50 drops are completed, raise the cylinder to eye level and read the volume of the material. A-3. A-3.1 CALCULATION Calculate the bulk density g/ml = G as follows: Bulk density, where m = mass in g of the material V = volume taken for the test, and in ml of the material after 50 tars. APPENDIX B [ Table 1, Item (xi) ] DETERMINATION B-l. B-l.1 REAGENTS Concentrated Hydrochloric Diamine Acid Tetra Acetic Acid ( EDTA ) OF CALCIUM OXIDE B-l.2 Standard Ethylene Solution - N/50. B-l.3 Murexide Indicator Buffer Hydroxide-Ammonium Chloride B-1.4 Ammonium chloride and 30 percent Solution - Mixture of 10 percent ammonium ammonium hydroxide in the proportion of 1 : 5. B-2. PROCEDURE B-2.1 Digest about 0.5 g of the sample in 10 ml of concentrated hydroFilter the solution after chloric acid in a IOO-ml beaker, on a water-bath. diluting it to 50 ml. Wash the residue collecting all the filtrate in a standard !250-ml flask. [ Preserve the residue for silica determination (see C-l.1 )]. Dilute the contents to 250 ml. Titrate 10 ml of this solution 7 IS : 9406 - 1980 against standard ethylene diamine tetra acetic acid ( EDTA ), solution using murexide as indicator and a mixture of ammonium chloride and ammonium hydroxide as buffer during titration. B-3. CALCULATION Calcium where volume in ml of standard EDTA solution titration, normality of the EDTA solution used, and N= taken for test. M = mass in g of the material V = oxide, percent by mass = 14.02 V.iV M used for the APPENDIX C [ Table 1, Ihm (xii) ] DETERMINATION C-l. PROCEDURE OF SILICA C-l.1 Transfer the residue on filter paper obtained in B-2.1 to a weighed dry platinum crucible and ignite at 700°C in a muffle furnace for 2 hours and re-weigh to get silica content. C-2. CALCULATION Silica where B = mass in g of the crucible M E= mass in g of the material B -A ( as SiOs ), percent by mass = M x 100 and residue taken after ignition, A =: mass in g of the empty crucible, and for test. APPENDIX D [ Table 1, Item (xiii) ] DETERMINATION D-l. D-I.1 ^___ REAGENTS Linseed Oil See IS : 75-1973*. OF OIL ABSORPTION *Specification for linseed oil raw and refined ( second rmision ). 8 IS: 9406 - 1980 D-2. PROCEDURE D-2.1 Place about 2 g of dry material accurately weighed, on a glazed porcelain, ground-glass or marble plate. Add linseed oil from a weighed dropping bottle, drop by drop, and regularly each drop being mixed well Incorporate the oil thoroughly in the with the material using a knife. course of 20 minutes, into the whole of the material with the knife, until Weigh the dropping bottle again and a coherent mass is obtained. determine by difference the mass of oil in grams. Where an approved sample is used for comparison, the oil absorption of the approved sample shall be determined by the same person and at the same time. D-3. CALCULATION 100 M M I D-3.1 Oil absorption, where g per 100 g = M = mass in g of linseed oil absorbed, and Ml = mass in g of the dry material taken for the test. APPENDIX E [ Tuble 1, Item (xiv) ] DETERMINATION OF SEDIMENTATION VOLUME in a stoppered graduated measuring Make up the volume to 50 ml with toluene, shake thoroughly cylinder. for 5 minutes and allow to stand for 1 hour. Measure the volume of the sediment. E-l. PROCEDURE E-l.1 Transfer 2 g of the material APPENDIX F [ Table 1, Item(xv) ] RETENTION F-l. PROCEDURE F-l.1 Transfer 20 g of the material to a measuring cylinder, add sufficient water to make volume up to 100 ml and shake vigorously for 2 minutes. Allow to stand. Draw sample after 5 minutes and 20 minutes by means of 25 ml pipette from a point 10 cm below the surface of the liquid. Determine the mass per millilitre of the sample of suspension removed by means of a pyknometer. 9 IN SUSPENSION IS : 9406 ( l 1980 Continued from pa@ 2 ) Representing Mambsrs Sturdia Chemicals Ltd, Bombay SHRI J. N. GHOSAL SARI H. C. VIJAYANATH ( Alternate ) Cosmos India Rubber Works Pvt Ltd, Bombay SHRIC. S. INAMDAR SHRI SIGN GUPTA ( Alfernafe ) National Rubber Manufacturers Ltd, Culcutta SHRI R. P. M~TI~UR Srrer A. K. BISWAS ( A&ernalc ) Camphor & Allied Products Ltd, Barcilly SHRI S. N. MEBTA SHY S. N. MEHRA ( Alternate j Bata India Ltd, Calcutta Sum S. C. NANDY SHR.I S. S~RKAR ( Alternate ) Travancore Titanium Products Ltd, Trivandrum DB V. S VIJAYAN NAYAR Synthetics and Chemicals Ltd, Bombay SHRI M. M. PATEL SHRI R. P. DUBEY ( Alternate ) Swastik Rubber Products Ltd, Pune SHRI V. D. PENDSE SHRI S. V. TATHAWADKAR ( Alternate ) I. A. & I. C. Pvt Ltd, Bombay SHRI P. S. PRATAP SHXI C. N. VYAS ( Alternate ) Philips Carbon Black Ltd, Calcutta SHRI R. ROY C~OWDRURY Da S. P. BASU ( Alternate ) Canara Rubber Products Pvt Ltd, Mangalore DR S. M. SRETTY Waldies Ltd, Calcutta SHRI D. V. WITTENBAKER SHRI A. DEB ( Alternate )